Method for drying polymeric materials

ABSTRACT

An improved extrusion dryer for drying wet polymeric materials comprises a compression zone where the wet material is compressed and heated and an expansion zone where the compressed hot material is allowed to expand and the volatile liquid to volatilize. The expanded material is conveyed by screw to an unrestricted outlet where it is separated from vapours and isolated in the dry form. The extrusion dryer of this invention operates at low temperatures and low power consumption and is suitable for drying at high throughput rates elastomeric polymers such as polybutadiene, butyl rubber, as well as heat sensitive polymers.

United States Patent 1191 [11] 3,834,440 McCracken Sept. 10, 1974 [54] METHOD FOR DRYING M RIC 3,280,090 10/1966 Scoggin .l 260 949 F T 3,367,635 2/1968 Gresch 259/4 MA ERIALS 3,395,746 8/1968 Szalo et al 1 159/47 R [75] nve tor: Na han Jo n cC ke a 3,476,736 11/1969 Kahre 260/96 x Ontario, Canada 3,477,491 11/1969 MacHenry et al. 159/2 E [73] Assignee: Polymer Corp-oration Limited 34/42 Samla, omarlo, Canada 1223,9421 2/1955 Fuller 159/2 E Filedi P 1972 FOREIGN PATENTS OR APPLICATIONS [21] Appl. NO; 289,567 734,182 7/1955 Great Britain 159/2 E Primary Examiner-Jack Sofer [52] US. Cl 159/47 R, 159/2 E A" A t s D & 51 1111.01. B01d 1/00, F26b 7/00, BOld 1/28 331? gen or evens er [58] Field of Search 159/2 E, DIG. I0, 47;

425/204, 208, 812 5 ABSTRACT An improved extrusion dryer for drying wet polymeric [56] References cued materials comprises a compression zone where the wet UNITED STATES PATENTS material is compressed and heated and an expansion 2,615,199 10/1952 zone where the compressed hot material is allowed to 2,719,325 10/1955 expand and the volatile liquid to volatilize. The ex- 2733951 H1956 panded material is conveyed by screw to an unrestricted outlet where it is separated from vapours and 3:025:565 3/1962 isolated in the dry form. 3,046,609 7/1962 Bergmeister et al 264/165 The extrusion dryer of this invention operates at low 3,067,462 12/1962 Kullgren 204/202 X temperatures and low power consumption and is 3,078,511 2/1963 Street 159/2 E suitable for at throughput rates g; EL W 59/2 E elastomeric polymers such as polybutadiene, butyl men a 3,222,797 12,1965 rubber, as well as heat sensitive polymers. 3,240,746 3/1966 Davis 260/415 9 Claims, 4 Drawing Figures DELIQUEFYING MACHINE VENT FLASH VAPOR /5 ii POLYMER ,Q

PATENTE SEH 0 I974 3.834.440 SHEET 1 OF 2 DELiQUEFYING MACHINE FLASH VAPOR POLYMER M 1 METHOD FOR DRYING POLYMERIC MATERIALS This invention relates to method and apparatus for BACKGROUND OF THE INVENTION In the production of synthetic polymers such as synthetic rubber, the material emerges from the polymerization process as a slurry of the material in water. Before the material can be baled or otherwise used, it must be dewatered and then dried to a moisture level of less than 1 percent. Drying is generally accomplished by one of two means: mechanical or tunnel dryers. In tunnel dryers, the material is passed through an enclosed, heated atmosphere where water freely evaporates and is drawn off, and the material emerges substantially dry. Mechanical dryers, as distinct from tunnel dryers, are often referred to as expander or extrusion dryers.

Present extrusion dryers work on the well-known worm-screw extrusion machine principle. They may be divided into single and multiple screw types. The former is exemplified in the apparatus described in US. Pat. No. 3,222,797. A multiple screw type dryer is described in Reissue Pat. No. 23,948, granted Feb. 15, I955. Differing somewhat in detail, single and multiple screw dryers are essentially similar in their basic machine elements and operation.

In the single screw machine, the dewatered material is advanced along a barrel by a worm-screw against a restriction such as a multi-orifice die. Against the restriction, a back-pressure is built up and, due to mechanical working by the screw, the temperature in the material is increased. Heat may also be added by means of steam jackets surrounding the barrel. Although the sensible heat within the material is normally sufficient to vaporize the liquid element in the material, the backpressure in the barrel is sufficient to prevent this occurring. Upon expulsion from the die into a zone of lower pressure, e.g., atmospheric pressure, flash vaporization takes place, the moisture escaping and rupturing the material into substantially dry crumb form.

In extrusion dryers of multiple screw type having two screws, for example, the material is advanced along a double barrel having contiguous parallel bores communicating via a central continuous slot, by twin wormscrews of opposite hand and rotation. At an intermediate position between an inlet at one end of the barrel and an outlet at the other end is a block valve comprising a block, slidably adjustable in a housing in communication with the bores and arranged to cooperate with blisters on the screws, generally known as compounders, to restrict flow and create a back-pressure in the material upstream of the valve. Downstream of the block valve is a low pressure zone which is vented to a low pressure source, e.g., atmosphere. Moisture from the evaporation taking place in this zone is vented off and the material is advanced to a single screw extrusion barrel where it is recompressed and at the same time reheated. Finally the material is expelled through die means where it forms a crumb and is conveyed away on a cooler/conveyor.

The electrical power requirements for extrusion dryers are approximately twice that of a tunnel dryer of similar capacity. More complicated in themselves and in their mode of operation, and operating as they do at high temperatures, extrusion dryers require complicated post-dryer equipment such as vibrating cooler/- conveyors. In consequence, maintenance costs of allmechanical systems can be as much as percent higher than tunnel dryer systems.

There are of course some important advantages in the use of extrusion dryers: the product is more uniform, freer from contamination and less floor space is required than for tunnel dryers. If the machine capacities can be increased, the operating temperatures reduced, the power requirements lowered and the severe mechanical problems associated with dryer and postdryer equipment can be alleviated, then mechanical drying systems prove superior over tunnel systems on all counts.

SUMMARY OF THE INVENTION It has been discovered that in drying polymeric materials in extrusion dryers, considerably improved results are obtained in a machine which includes an adjustable, variable-flow restriction downstream of the inlet for creating a back-pressure in the material and a continuation bore and conveying means downstream of the restriction having an unrestricted outlet in communication with ambient atmosphere.

According to the present invention therefore there is provided a method of drying an extrudable polymeric material containing volatile material in an extruder comprising a number of zones which method comprises:

l. compressing the material in a zone maintained at a temperature capable of vaporizing the volatile liquid at atmospheric pressure and a pressure sufficient to prevent such vaporization;

2. forcing said compressed material through a restriction into an expansion zone maintained at reduced pressure whereby said liquid is vaporized and said polymeric material expanded; and

3. conveying said expanded material and vaporized liquid through the expansion zone wherein the vapor separates from said material.

In the utilization of the apparatus and method of the invention, the peak product temperatures of the extrudable material in the dryer and residence time at these temperatures have been reduced so as to enable more heat sensitive products to be successfully dried, and the throughput capacity of the dryer has been markedly increased over the capacity of the prior art extruders of the same size. Excessive mechanical stresses in the dryer have been eased because when running the machine at or close to capacity the power requirements of the machine are reduced. Finally, the residual temperature of the product leaving the dryer has been lowered.

Other advantages will be apparent to those skilled in the art from reading the following description taken in conjunction with the accompanying drawings in which like reference characters refer to like parts throughout the several views and in which:

DESCRIPTION OF THE DRAWINGS FIG. 1, is a diagrammatic representation of the apparatus of the present invention with associated equipment in a rubber drying process;

FIG. 2, is a simplified plan view in section showing the apparatus of the invention;

FIG. 3, is a side elevation of the apparatus shown in FIG. 2; and

FIG. 4, is a cross-sectional elevation taken along the line 44 in FIG. 3.

DETAILS OF THE INVENTION Referring to FIG. 1 there is shown an extrusion drying according to the invention generally indicated at 10. To the right of the extrusion dryer is represented a deliquefying machine 11 which may be of the extrusion type shown or it may be equipment of any other wellknown type adapted to reduce the liquid content of a slurry or synthetic rubber or other polymeric material to not more than 15 percent by weight and preferably to between 5 and 8 percent. The machine 11 is arranged to feed the deliquefied material into a hopper 12 of the dryer while an outlet 13 discharges the dried material onto a cooler/conveyor 14 represented as a belt-type conveyor but which may be of the vibrator or any other type.

Referring now more particularly to FIG. 2 through 4, a double-barrelled structure 15 is fabricatedto define two parallel bores 16 and 16a formed so that they communicate with each other through a common slot 17 (FIG. 4) running the length of the barrel structure. Surrounding the barrel structure is a continuous sheath 18 spaced from the barrel structure and compartmented by transverse bulkheads such as 19 to provide a series of heating or cooling jackets 20 adapted to receive a flow of fluid such as steam or water or any other heat transfer medium from an exterior system.

Adjacent one end of the barrel structure remote from outlet 13 is a gravity feed inlet 21 surmounted by hopper 12 whereby particulate deliquefied material is fed to the bores 16 and 16a. Between the inlet 21 and the outlet 13 is a pressure block-valve indicated at 22. The valve will be more full described later herein.

Freely rotatable within the bores 16 and 16a are oppositely handed worm-screws 23 and 23a. Except for the handing of the flights, the worm-screws are precisely similar. They are preferably synchronized so that their flight crests are contiguous. The screws rotate in opposite directions: screw 23 in an anti-clockwise direction and screw 23a in a clockwise direction when viewed at the outlet 13. The screws are driven by power means such as an electric motor through a suitable transmission. The power means is generally indicated at 24.

The screws are designed to increase the pressure ratio up to valve 22 and this is done by gradually increasing the stem diameter and decreasing the pitch of the screw flights in well known manner. At valve 22, the screw stems are increased to form blisters 25 and 25a. These blisters carry multiple-start, shallow, reverse flights 26 and 26a on their peripheral surfaces. That is to say, flights 26 are of opposite hand to the main worm-screw 23 and flights 26a are of opposite hand to main worm-screw 23a. These blisters are sometimes referred to as compounders and there is a small running clearance between their flight crests and the barrel bores for a maximum flow restriction.

lntegrally formed on the upper side of the barrel structure normal to the axes of the barrel bores is a hollow rectangular housing 27 which opens into the bores 16 and 16a. The housing carries a sliding valve block 28 with arcuate lower surfaces 29 and 29a which are flush with the surfaces of bores 16 and 160 respectively when the block 28 is in its fully lowered'position. The

' position of the block 28 is adjustable with respect to the the fully lowered position to a position sufficiently removed from the blisters such that the material is allowed to by-pass the normal restriction of the blisters. By this means, therefore, is controlled the backpressure in the. material upstream of the block valve. Adjustability is effected by a screw 30 rotatably anchored to the valve block at 31 and threadibly engaging a member 32 bridging the top of valve housing 27. The screw is operated by a handwheel 33 and locked at the selected setting by a locknut 34.

Barrel structure 15 extending downstream of valve 22 is precisely similar to the structure upstream of the valve and is merely a continuation thereof. The block valve 22 defines a restriction zone 35 and divides the barrel structure into a high pressure compression zone 37, preceded by a feed zone 36, upstream of the valve and an expansion zone 38 downstream thereof. The flighted screws in expansion zone 38 are of constant pitch and stem diameter and, since in this portion of the machine the screws only have a conveying function, a lighter form of construction, e.g., sheet metal fabrication or machining from light alloy instead of steel alloy, may be used.

The dual screw extrusion dryer described hereinabove represents but one embodiment of the apparatus of this invention. It is also possible to use a single screw extrusion dryer having a compression zone and an expansion zone provided with an unrestricted outlet for dry material and vapours and an adjustable restriction zone between said compression and expansion zones.

Operation of the extrusion dryer according to the present invention will be described by way of specific examples and the performance figures compared with performance figures obtained from a similar machine constructed in accordance with the known art.

Example 1 An aqueous slurry of 98 percent cis l ,4 polybutadione having a Mooney viscosity (MIL-4 212F) of 40 was dewatered in the dewatering machine 11 to about 6 percent moisture content and fed to the hopper 12 of the extrusion dryer 10. For start-up, heat was built up in the barrel structure by passing steam through the heating jackets 20 and the valve block 28 was partly backed off. Material entering the bores 16 and 16a through inlet 21 was conveyed therealong by screws 23 and 23a and by-passed the blisters 25 and 25a at the block valve 22. The block 28 was progressively closed down, to restrict the passage of the material and create an increasing back-pressure therein. This backpressure was increased until a barrel temperature of between 300-350F was reached. The heat from mechanical working of the material in the compression zone was sufficient for the drying process. Small amounts of steam were added during the operation to balance the heat loss by radiation. The back-pressure in the compression zone 37 varied from about 750 to about 2,500 psi.

The back-pressure built up in the material in the compression zone was sufficient to prevent evaporation of the water present in the material. Some water was expelled from the material and was forced back along the bores towards the inlet. As the pressure in the material upstream reduced, so this water evaporated and escaped through the inlet 21 and hopper 12 to atmosphere. The polybutadiene material was expelled from block valve 22 into the 'continuations of bores- 16 and 16a where the pressure was considerably lower than that upstream of the valve and very close to atmospheric pressure. Rapid evaporation of the residual water present in the dewatered material caused the material to expand and rupture into crumb form. The material was then conveyed along the continuation bores by the screws with continued formation of water vapour, which finally escaped over the crumb to atmosphere at the outlet 13. The material issued from the outlet 13 at a temperature of about 270F, and was conveyed on the cooler/conveyor system 14 to baling machines. The final moisture content was about 0.3 percent.

A dual screw 6-inch extrusion dryer provided with a 500 HP drive means and operated in accordance with the present invention yielded up to 9,000 lbs. of dry polybutadiene product per hour using only 300 of the available HP of the drive means. Productivity rates of this order of magnitude were maintained over prolonged periods of operation so that the production/- power ratio was in the order of about 30 lbs. of product per HP per hour.

The same extrusion dryer having an additional single screw section at the outlet end and operated with a die at the outlet, i.e., not in accordance with this invention, delivered up to 3,500 lbs/hr. steady production at almost full power. Barrel temperature was between 390 430F, resulting in scorching and even ignition of the dried polymer at the outlet. Average productivity was in the order of a ratio of 7 lbs. of product per HP per hour. The temperature of the extrudate was reduced to a level of about 350F by venting off the volatile material downstream of the restriction; unfortunately it resulted in a loss through the vent system of nearly 1,000 lbs/hr of the polybutadiene material in the form of fines.

Example 2 Three extrusion drying runs were carried out on different polymers using the procedure and the dual screw extrusion dryer as described in Example 1. The polymers, all dewatered to a moisture level of 5-8 percent, were as follows:

A. a masterbatch of 100 parts of cis-l ,4 polybutadiene and 37.5 parts of a highly aromatic extender oil having a Mooney viscosity (MIL-4' 212F of 36;

B. a butyl rubber having a Mooney viscosity (M/L8 2l2F) of 45 and an unsaturation level of 0.7 mol. percent; and

C. a brominated butyl rubber containing 2.0 percent bromine and having a Mooney viscosity (MIL-4' 257F) of 51.

The data are shown in the table below .tleeif e Final moisture (71) 0.3 0.3 0.75 Av. power consumption (HP) 200 220 200 Av. throughput (lbs/hr) 7000 6000 4000 Av. throughput/power ratio 30 27 20 All these runs indicated that various polymers could be effectively'dried at high rates at safe peak temperatures.

A comparative experiment was carried out with polymer C using a conventional dual screw extrusion dryer. The temperature in the barrel rose to about 350F at which temperature the polymer degraded a scorched black mass.

What is claimed is:

l. A method of drying an extrudable polymeric material containing a volatile liquid in an extrusion dryer comprising a number of elongated zones serially interconnected within a continuous barrel structure, which method comprises:

a. introducing said material into a feed zone;

b. compressing said material in a compression zone maintained at a temperature capable of vaporizing said volatile liquid at atmospheric pressure and a pressure sufficient to prevent such vaporization;

c. forcing said compressed material through a restriction zone into an expansion zone;

-d. conveying said material through the expansion zone while subjecting it to ambient atmospheric pressure through said unrestricted terminal outlet of the expansion zone whereby most of said liquid is rapidly vaporized and said material is expanded and ruptured into crumb in commingled relationship; and

e. discharging all of said crumb and said vaporized liquid through said unrestricted outlet of said ex pansion zone and separating said crumb and said vaporized liquid.

2. The method of claim 1 wherein the volatile liquid comprises water.

3. The method of claim 2 wherein the amount of water in said polymeric material introduced into the feed zone is between about 5 and 8 percent by weight.

4. The method of claim 2 wherein the extrudable polymeric material is a high molecular weight elastomeric material.

5. The method of claim 4 wherein the elastomeric material is butyl rubber or a halogenated derivative of butyl rubber.

6. The method of claim 1 wherein the material is maintained in the compression zone at a temperature of between 300350F.

7. The method of claim 6 wherein the material is heated by mechanical working in the compression zone.

8. The method of claim 1 wherein the polymeric material issues from the expansion zone in the form of crumb at a temperature of less than 300F.

9. The method of claim 8 wherein the elastomeric material is a polymer of a conjugated diolefin.

UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent 3, 834,440 Dated September 10, 1974 Inventor(s) Nathan John MCCRACKEN It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:

IN THE CLAIMS:

Claim 1, sub-paragraph (c) after "zone" second occurrence, and before the semi-colon insert:

- having a single unrestricted terminal outlet of a cross-section nbtless than the polymeric'material path of the expansion zone Signed and sealed this 10th day of December 1974.

(SEAL) Attest:

mccoy M. GIBSON JR. c. MARSRALL DANN Attesting Officer Commissioner of Patents 'IQRM po'wso (wss) USCOMM-DC 00370-959 i 0.5. GOVIRNNENT PRINTING OFFICE: l9! 0-3'i-l3l. 

2. The method of claim 1 wherein the volatile liquid comprises water.
 3. The method of claim 2 wherein the amount of water in said polymeric material introduced into the feed zone is between about 5 and 8 percent by weight.
 4. The method of claim 2 wherein the extrudable polymeric material is a high molecular weight elastomeric material.
 5. The method of claim 4 wherein the elastomeric material is butyl rubber or a halogenated derivative of butyl rubber.
 6. The method of claim 1 wherein the material is maintained in the compression zone at a temperature of between 300*-350*F.
 7. The method of claim 6 wherein the material is heated by mechanical working in the compression zone.
 8. The method of claim 1 wherein the polymeric material issues from the expansion zone in the form of crumb at a temperature of less than 300*F.
 9. The method of claim 8 wherein the elastomeric material is a polymer of a conjugated diolefin. 